HRID1910519

反应详情

EQUATION

反应方程式

HRID 1910519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Oxalyl dichloride (141 μl, 1.67 mmol) was added dropwise to a solution of 1-methylpiperidine-4-carboxylic acid hydrochloride (300 mg, 1.67 mmol) in DCM (20 ml) and few drops of DMF (catalytic amount). The reaction was stirred at room temperature for 2 hours. The volatiles were removed under vacuum, and the crude was taken up with pyridine (20 ml). 1,2-Diphenylethanol (331 mg, 1.67 mmol) was added, and the resulting suspension was heated under microwave irradiation at 140° C. for 1 hour. Pyridine was removed under vacuum, and the crude was purified by flash chromatography (DCM/MeOH=97/3 to 94/6) to obtain 1,2-diphenylethyl 1-methylpiperidine-4-carboxylate (200 mg).

WORKUP

后处理

  1. customThe volatiles were removed under vacuum
  2. temperaturethe resulting suspension was heated under microwave irradiation at 140° C. for 1 hour
  3. customPyridine was removed under vacuum
  4. customthe crude was purified by flash chromatography (DCM/MeOH=97/3 to 94/6)